The stability of beta-CD . C7H8O . 5H2O was investigated using TG and DSC. The weight loss takes place in three stages : the dehydration occurs at 47-110-degrees C; the dissociation of beta-CD . C7H8O occurs at 200-250-degrees C; and the decomposition of beta-CD begins at 270-degrees C. The kinetics of the dehydration of beta-CD . C7H8O . 5H2O and the dissociation of beta-CD . C7H8O in a dry nitrogen flow were studied by means of thermogravimetry, both at constant temperature and with linearly increasing temperatures. The dehydration of beta-CD . C7H8O . 5H2O is dominated by a three-dimensional phase boundary reaction, R3. The activation energy E is 101.75 kJ mol-1. The pre-exponential factor A is 9.502 x 10(10) min-1. The dissociation of beta-CD . C7H8O is affected by a two-dimensional diffusion process, D2. The activation energy E is 158 kJ mol-1. The pre-exponential factor A is 3.3 x 10(14) min-1. Scanning electron microscope observation and crystal structure analysis are in good agreement with the results obtained from thermogravimetry.